A novel ToF-SIMS operation mode for sub 100nm lateral resolution: Application and performance

Kubicek, Markus; Holzlechner, Gerald; Opitz, Alexander Karl; Larisegger, Silvia; Hutter, Herbert; Fleig, Jürgen

doi:10.1016/j.apsusc.2013.10.177

Cited by 79 publications

(53 citation statements)

References 40 publications

(49 reference statements)

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“…The voltage-induced high electron concentration in the electrolyte may even lead to an extension of the oxygen incorporation area from the triple phase boundary of Pt electrodes along parts of the free electrolyte surface; this was reported for YSZ electrolytes under strong cathodic bias in Ref. 38.…”

Section: Comparison With Literature Data On Partial Conductivities Ofmentioning

confidence: 71%

Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals

Rupp

Głowacki

Fleig

2016

J. Electrochem. Soc.

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The defect chemistry and charge transport properties of La 0.95 Sr 0.05 Ga 0.95 Mg 0.05 O 3-δ (LSGM) single crystals, grown by the Czochralski technique, were studied by impedance spectroscopy performed over a wide temperature range (180-800 • C) and oxygen partial pressures from 0.21 to 1013 mbar. Owing to ion blocking Pt thin film electrodes impedance data showed a Warburg type 45 • slope in the complex impedance plane. The spectra were analyzed by means of a generalized transmission line model which yielded the electronic and ionic conductivity, chemical and dielectric capacitance and the oxygen chemical diffusion coefficient. Activation energies for electronic (0.89 eV) and ionic charge transport (0.95 eV at low and 0.56 eV at high temperatures) were determined. Oxygen partial pressure dependent measurements revealed that the p-type conductivity is exactly proportional to p O 2 1/4 and that the ionic transference number approaches 1 for low oxygen partial pressures and low temperatures. Additional Hebb-Wagner type DC polarization experiments were carried out to determine the n-and p-type conductivities in a broad chemical potential range and to verify the results obtained by the AC impedance measurements. Strontium and magnesium doped lanthanum gallate (LSGM) has been widely investigated as potential electrolyte material in solid oxide fuel cells (SOFC) and thus as promising alternative to the fluorite type electrolytes yttria stabilized zirconia (YSZ) and gadolinium doped ceria (GDC). At lower temperatures (<700• C) the ionic conductivity of LSGM can exceed the conductivity of YSZ by more than a factor of 5 1-3 . Although the ionic conductivity below ca. 600• C is smaller compared to GDC, LSGM has the advantage of a broad electrolytic domain with negligible electronic conductivity under typical reducing and oxidizing conditions of SOFCs.4,5 However, electrochemical properties of LSGM have been investigated almost exclusively on polycrystalline samples, 1,6-11 in contrast to YSZ where many studies are also available on single crystals. This is largely because of the difficulty to synthesize larger single crystals of the preferred composition La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 3-δ with sufficient quality. The very few existing studies on LSGM, mostly with lower dopant concentration, dealt with crystal structure, thermal conductivity and ionic conductivity. 7,12 Detailed information on the electronic conductivity of LSGM single crystals is not available so far.Measurements on polycrystalline materials often suffer from difficulties to discriminate between effects induced by grains and grain boundaries. In principle, impedance spectroscopy allows separation of resistive grain and grain boundary contributions and often a brick layer model is used for data analysis. [13][14][15] However, this approach only works at lower temperatures (due to the limited frequency range of impedance spectroscopy) and for the total conductivity, which is largely ionic in LSGM. A separation of resistive bulk and grain boundary contributi...

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Section: Comparison With Literature Data On Partial Conductivities Ofmentioning

confidence: 71%

Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals

Rupp

Głowacki

Fleig

2016

J. Electrochem. Soc.

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“…To obtain 18 O depth profiles, a TOF.SIMS 5 instrument (ION‐TOF, Münster, Germany) was used with a pulsed bismuth primary ion gun (25 keV, Bi 1 + ) working in the “Collimated Burst Alignment” (CBA) mode . Applying the CBA mode enables an accurate determination of oxygen isotopic fractions and an improved lateral resolution.…”

Section: Methodsmentioning

confidence: 99%

Oxygen Ion Conduction in Bulk and Grain Boundaries of Nominally Donor‐Doped Lead Zirconate Titanate (PZT): A Combined Impedance and Tracer Diffusion Study

et al. 2015

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Oxygen ion conduction in Nd 3+ -doped Pb(Zr x Ti 1 -x )O 3 (PZT) was investigated by impedance spectroscopy and 18 O-tracer diffusion with subsequent secondary ion mass spectrometry (SIMS) analysis. Ion blocking electrodes lead to a second relaxation feature in impedance spectra at temperatures above 600°C. This allowed analysis of ionic and electronic partial conductivities. Between 600°C and 700°C those are in the same order of magnitude (10-4 S/cm) though very differently activated (2.4 eV vs. 1.2 eV for ions and electron holes, respectively). Oxygen tracer experiments showed that ion transport mainly takes place along grain boundaries with partly very high local ionic conductivities. Numerical analysis of the tracer profiles, including a near-surface space charge zone, revealed bulk and grain-boundary diffusion coefficients. Calculation of an effective ionic conductivity from these diffusion coefficients showed good agreement with conductivity values determined from impedance measurements. Based on these data oxygen vacancy concentrations in grain boundary and bulk could be estimated. Annealing at high temperatures caused a decrease in the grain-boundary ionic conductivity and onset of additional defect chemical processes near the surface, most probably due to cation diffusion.

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“…The measurements were carried out on a TOF-SIMS IV instrument (ION-TOF GmbH, Muenster, Germany). A pulsed bismuth primary ion gun (25 keV, Bi 3 þ þ ) was used in the "collimated burst alignment" (CBA) mode enabling high lateral resolutions below 100 nm [18,27]. Additionally, to ToF-SIMS imaging in the CBA mode, high mass resolution spectra were acquired using the high current bunched mode (HCBU) to differentiate contributions of H 2 À and D À and OH 2 À and OD À secondary ions (SI) to the peaks at m/z ¼ 2 and m/ z¼18, respectively.…”

Section: Time-of-flight Secondary Ion Mass Spectrometry (Tof-sims)mentioning

confidence: 99%

“…Nishimoto et al [17] detected hydrogen in the ferritic grains by SIMS using a cryogenic sample holder. State-of-the-art ToF-SIMS instruments may provide precise element and phase mappings with a lateral resolution below 100 nm [18], enabling imaging of the microstructure and analysis of its phase dependent chemical composition [13,14,19]. Recently, ToF-SIMS image analysis has substantially been improved by multivariate analysis (MVA) of image data and by data fusion of the chemical and topographic information [14].…”

Section: Introductionmentioning

confidence: 99%

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel micro-structure

Sobol

Holzlechner

Nolze

et al. 2016

Materials Science and Engineering: A

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A novel ToF-SIMS operation mode for sub 100nm lateral resolution: Application and performance

Cited by 79 publications

References 40 publications

Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals

Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals

Oxygen Ion Conduction in Bulk and Grain Boundaries of Nominally Donor‐Doped Lead Zirconate Titanate (PZT): A Combined Impedance and Tracer Diffusion Study

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel micro-structure

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A novel ToF-SIMS operation mode for sub 100nm lateral resolution: Application and performance

Cited by 79 publications

References 40 publications

Electronic and Ionic Conductivity of La0.95Sr0.05Ga0.95Mg0.05O3-δ(LSGM) Single Crystals

Electronic and Ionic Conductivity of La0.95Sr0.05Ga0.95Mg0.05O3-δ(LSGM) Single Crystals

Oxygen Ion Conduction in Bulk and Grain Boundaries of Nominally Donor‐Doped Lead Zirconate Titanate (PZT): A Combined Impedance and Tracer Diffusion Study

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel micro-structure

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Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals

Electronic and Ionic Conductivity of La_0.95Sr_0.05Ga_0.95Mg_0.05O_3-δ(LSGM) Single Crystals